Method for preparing magic number cluster nanocrystal in indirect mode of ion exchange
A technology of ion exchange and nanocrystals, which is applied in the preparation of cadmium compounds, lead compounds, nanotechnology, etc., can solve the problems of low yield and purity of semiconductor nanocrystal products, achieve improved atom utilization, simple operation, good stability effect
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Embodiment 1
[0049] Example 1 Synthesis of cadmium selenide (CdSe) magic number cluster nanocrystals
[0050] Raw materials: cadmium oxide (CdO), oleic acid (OA), zinc oxide (ZnO), selenium powder (Se), trioctylphosphine (TOP), octadecene (ODE), octylamine (OTA) are all from Aldrich; Cyclohexane (CH) was from Tianjin Zhiyuan Reagent Co., Ltd.
[0051] Testing instrument: TECHCOMP UV 2310Ⅱ ultraviolet spectrophotometer is Shanghai Tianmei Technology Instrument.
[0052] (1) Referring to the aforementioned documents, according to the method and requirements for preparing ZnSe conventional nanocrystals (ZnSe RNCs):
[0053] (i) Weigh 0.4883g ZnO, 3.729g OA (oleic acid) and 5g ODE into a three-necked round-bottomed flask, switch between vacuum and nitrogen at 40°C for more than three times, wait until the bubbles disappear and slowly raise the temperature to 120°C, and keep vacuum heating 1h, change to N 2 The atmosphere was heated up to 290°C for 2 hours (the solution was clear and transpa...
Embodiment 2
[0059] Example 2 Synthesis of lead selenide (PbSe) magic number cluster nanocrystals
[0060] Raw materials: lead oxide (PbO), oleic acid (OA), zinc oxide (ZnO), selenium powder (Se), trioctylphosphine (TOP), octadecene (ODE) are all from Aldrich; cyclohexane (CH) From Tianjin Zhiyuan Reagent Co., Ltd.
[0061] Testing instrument: TECHCOMP UV 2310Ⅱ ultraviolet spectrophotometer is Shanghai Tianmei Technology Instrument.
[0062] Preparation:
[0063] (1) Synthesize ZnSe according to the same method as in Example 1;
[0064] (2) Test the dispersion of 15 μL of sample into 3 mL of dispersant (2 mL of cyclohexane-1 mL of octylamine mixed solvent) with a UV-visible spectrophotometer. It can be seen that in the octylamine-cyclohexane mixed solution, the sample immediately has the 299nm characteristic absorption peak of the ZnSe magic number nanocluster to appear, as figure 1 As shown, it can be judged that the ZnSe magic number cluster nanocrystal intermediate was obtained unde...
Embodiment 3
[0067] Example 3 Synthesis of cadmium sulfide (CdS) magic number cluster nanocrystals
[0068] Raw materials: cadmium oxide (CdO), oleic acid (OA), zinc oxide (ZnO), sulfur powder (S), octadecene (ODE) are all from Aldrich; cyclohexane (CH) is from Tianjin Zhiyuan Reagent Co., Ltd.
[0069] Testing instrument: TECHCOMP UV 2310Ⅱ ultraviolet spectrophotometer is Shanghai Tianmei Technology Instrument.
[0070] Preparation:
[0071] (1) According to the method and requirements of preparing ZnS conventional nanocrystals (RNCs), the Zn precursor (Zn(OA) 2 ), and the Cd precursor (Cd(OA) 2 ) stock solution raw material B.
[0072] Take 2.2mL of Zn(OA) of raw material A 2 and 3.158g of ODE were placed in a 50mL three-necked round bottom flask, and the vacuum-nitrogen gas was switched at 40°C for more than three times. After the bubbles disappeared, the temperature was raised to 80°C, and the vacuum was kept for 30min, and then switched to N 2 Warm up to 120°C under atmosphere, c...
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